WO2011071064A1 - 有機薄膜の成膜装置および有機材料成膜方法 - Google Patents

有機薄膜の成膜装置および有機材料成膜方法 Download PDF

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Publication number
WO2011071064A1
WO2011071064A1 PCT/JP2010/071980 JP2010071980W WO2011071064A1 WO 2011071064 A1 WO2011071064 A1 WO 2011071064A1 JP 2010071980 W JP2010071980 W JP 2010071980W WO 2011071064 A1 WO2011071064 A1 WO 2011071064A1
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Prior art keywords
vapor
organic material
film forming
film
trap
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PCT/JP2010/071980
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English (en)
French (fr)
Japanese (ja)
Inventor
敏夫 根岸
弘 藤本
秀行 平岩
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株式会社アルバック
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Priority to KR1020127014728A priority Critical patent/KR101379646B1/ko
Priority to JP2011545224A priority patent/JP5474089B2/ja
Priority to CN201080055842.7A priority patent/CN102639746B/zh
Publication of WO2011071064A1 publication Critical patent/WO2011071064A1/ja

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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/12—Organic material
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/246—Replenishment of source material
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
    • C23C14/564—Means for minimising impurities in the coating chamber such as dust, moisture, residual gases

Definitions

  • the present invention relates to an organic thin film forming apparatus, and more particularly to a film forming apparatus and an organic material film forming method for heating and evaporating a material little by little.
  • Organic thin films to which light-emitting materials made of organic substances are added emit light with a color depending on the type of light-emitting material when an electric current flows in the film thickness direction. Recently, display devices and illumination devices using organic thin films Has been put into practical use and has been mass-produced.
  • the optimal content is determined.
  • the vapor arrival speed of one organic material fluctuates, the content rate changes, and the content rate in the film thickness direction fluctuates. If a portion that does not have the optimum content for light emission is formed, the light emission amount of the light emitting layer is reduced.
  • a film forming apparatus in which when an organic material used for film formation is heated and evaporated little by little, the vapor amount of the organic material released from the discharge apparatus is constant.
  • a film forming apparatus capable of recovering and reusing an organic material from vapor not used for film formation is provided.
  • the present invention provides a film formation tank in which an object to be formed is disposed, a vapor generation device that generates vapor of an organic material, and the vapor generated by the vapor generation device.
  • An organic thin film forming apparatus in which the vapor is discharged into the film forming tank from a discharge port formed in the discharging apparatus, wherein the vapor generating apparatus
  • a material supply device for supplying a material
  • an evaporation device for supplying the organic material from the material supply device to evaporate the organic material
  • a buffer unit for depositing and re-evaporating the vapor generated in the evaporation device
  • a buffer temperature control device for controlling the temperature of the buffer unit, the vapor generated by the evaporation device is supplied to the discharge device through the buffer unit, and the organic thin film is applied to the film formation target Film forming equipment It is.
  • the present invention is a film forming apparatus having a plurality of the steam generating apparatuses.
  • the present invention includes a film thickness monitor that detects a part of the vapor emitted from the buffer unit, and the buffer temperature control device controls the temperature of the buffer unit based on the detection value of the film thickness monitor.
  • this invention is a film-forming apparatus with which the said material supply apparatus rotates the axis
  • the present invention is the film forming apparatus, wherein the evaporation apparatus includes a material supply amount measuring unit that measures the amount of the organic material supplied from the material supply apparatus.
  • the material supply amount measuring means includes a receiving member that receives the organic material supplied from the material supply device, and a temperature measurement analyzer that calculates the supply amount of the organic material from a temperature change of the receiving member.
  • a film forming apparatus the buffer unit is formed of a plurality of thin metal wires, the thin metal wires partially overlap each other, and a flow path is formed by a gap between the thin metal wires and the thin metal wires.
  • the present invention is the film forming apparatus in which the buffer unit is configured by a plurality of nets, and a flow path is formed in a gap between the nets of the nets.
  • the number of meshes per unit area of the first mesh among the plurality of meshes is a second mesh positioned on the downstream side of the first mesh of the steam flowing in the buffer unit.
  • the number of meshes per unit area is less than the number of meshes.
  • the present invention is a film forming apparatus in which a backflow prevention gas supply device for supplying a backflow prevention gas is connected to the material supply device.
  • the steam generation device is configured such that the traveling direction of the steam that has passed through the buffer unit is a first direction that is inside the discharge device, and a second direction that is not inside the discharge device. It is the film-forming apparatus which has the switching apparatus switched between.
  • the steam generating device includes a trap device in which a trap part in contact with the steam is disposed inside the trap tank, and the trap tank is configured to be evacuated, and the trap part is evaporated.
  • a low-temperature apparatus that cools the trap temperature to a temperature lower than the temperature, and the second direction is a film-forming apparatus provided inside the trap tank.
  • the present invention also includes a film formation tank in which a film formation target is disposed, a vapor generation apparatus that generates vapor of an organic material, and a discharge apparatus that is supplied with the vapor generated by the vapor generation apparatus.
  • An organic thin film forming apparatus in which the vapor is discharged into the film forming tank from a discharge port formed in the discharge apparatus, wherein the vapor generating apparatus supplies the organic material
  • a supply device, an evaporation device for evaporating the organic material supplied from the material supply device, and a trap part in contact with the vapor are arranged inside the trap tank, and the inside of the trap tank is configured to be evacuated.
  • the steam generation device includes a film thickness sensor, the steam generation device generates a part of the steam before reaching the switching device, the film thickness sensor, A film forming apparatus configured to grow the organic thin film on a film thickness sensor.
  • this invention is a film-forming apparatus which has the said some vapor generating apparatus connected to the said said discharge
  • the present invention is a film forming apparatus in which the organic materials having different chemical structures are arranged in the material supply apparatuses of the plurality of vapor generation apparatuses.
  • this invention is a film-forming apparatus from which the said organic material arrange
  • the discharge device is connected to an evaporation container in which an auxiliary material that is an organic compound contained in a smaller amount than the organic material is disposed in the organic thin film, and the vapor of the auxiliary material is The film forming apparatus is configured to be introduced into the discharge apparatus at a lower introduction speed than the vapor of the organic material.
  • the present invention includes a sub trap device in which a trap portion in contact with the vapor of the sub material is disposed inside the trap tank, and the inside of the trap tank is configured to be evacuated.
  • the generated vapor of the secondary material is a film forming apparatus configured to be switched to be introduced into the discharge device and the secondary trap device. Further, the present invention supplies an organic material to the heating unit at a predetermined rate, generates steam, introduces the steam into the buffer unit, precipitates the organic material in the buffer unit, and deposits the organic material deposited in the buffer unit.
  • This is an organic material film forming method in which re-evaporation is performed and the re-evaporated vapor is discharged to a substrate to form a film.
  • the present invention is an organic material film forming method in which a part of the vapor derived from the buffer unit is measured, and the temperature of the buffer unit is controlled based on the measured value.
  • the temperature of the buffer unit is lowered from the evaporation temperature of the organic material so that the vapor is deposited in the buffer unit when the substrate is replaced, and is deposited in the buffer unit during film formation on the substrate.
  • the temperature of the buffer unit is raised above the evaporation temperature of the organic material so that the organic material re-evaporates.
  • the composition of the film thickness direction of the organic thin film with which multiple types of organic material was mixed can be made constant.
  • an organic thin film having a constant quality in the film thickness direction can be obtained.
  • steam conventionally discarded can be collect
  • the internal side view for demonstrating the film-forming apparatus of the 1st example of this invention Drawing for explaining the positional relationship of a plurality of vapor generators of the film forming apparatus
  • the internal side view for demonstrating the film-forming apparatus of the 2nd example of this invention The internal side view for demonstrating the film-forming apparatus of the 3rd example of this invention
  • FIGS. 1 and 2 represents a film forming apparatus of the first example of the present invention.
  • FIG. 1 is a cross-sectional view of the film forming apparatus 2 when viewed from the side
  • FIG. 2 is an internal layout view viewed from above.
  • the film forming apparatus 2 includes a film forming tank 11 and a discharge device 12.
  • a plurality of vapor generating devices 13 a, 13b are connected.
  • the steam generators 13a and 13b have the same internal structure here.
  • the steam generators indicated by reference numeral 13 show the interiors of the two steam generators 13a and 13b together.
  • the steam generators 13 a and 13 b are connected to the end portion on the same side in the longitudinal direction of the discharge device 12, but even if connected to the same end portion, one and the other are connected to the opposite end portion. It may be.
  • the film formation tank 11 is provided with a carry-in port 81 and a carry-out port 82 that are opened and closed when the film formation target 15 is carried in and out.
  • the carry-in port 81, the carry-out port 82, and a partition valve 29 described later are closed, the vacuum exhaust system 19 is operated, and the inside of the film forming tank 11 is evacuated to make a vacuum atmosphere.
  • the vacuum exhaust system 19 is continuously operated to evacuate the inside of the film forming tank 11.
  • the discharge device 12 includes a main body portion 35 and a discharge plate 36 that closes the opening of the main body portion 35.
  • a plurality of discharge ports 37 are formed in the discharge plate 36.
  • the discharge device 12 is disposed in the film formation tank 11, and the inside of the discharge device 12 is evacuated by the vacuum exhaust system 19 through the discharge port 37.
  • An organic material having the same or different chemical structure is disposed in each of the steam generators 13a and 13b.
  • one is an organic compound of an organic thin film base material (material constituting the organic thin film), and the other is a dopant contained in the organic thin film of the base material (for example, a light emitting material).
  • the content is different, and the organic compound of the base material and the organic compound of the dopant are separated from the base material in the separate steam generators 13a and 13b.
  • the vapor generating devices 13a and 13b can be operated simultaneously to co-deposit the base material and the dopant.
  • different materials can be arranged in the steam generators 13a and 13b and operated separately to form a laminated film.
  • Each of the steam generation devices 13a and 13b is configured to generate a vapor of the disposed organic material and supply it to the same discharge device 12.
  • the discharge device 12 is configured to discharge the vapor supplied from each of the vapor generation devices 13a and 13b into the film formation tank 11 from another discharge port 37 for each type of organic material, or the main body.
  • a cavity is formed in the part 35, and the steam generated by each of the steam generators 13 a and 13 b is supplied to the same cavity, mixed in the cavity, and discharged from the discharge ports 37 into the film formation tank 11. It is configured.
  • the discharge device 12 has the main body 35 and the discharge plate 36 disposed inside the film formation tank 11. However, if the airtightness of the film formation tank 11 is maintained, the discharge plate 36 is formed. A part or all of the main body 35 can be disposed outside the film formation tank 11 while being positioned inside the film formation tank 11.
  • a moving device 17 is disposed above the discharge device 12 in the film formation tank 11. Inside the film formation tank 11, a substrate disposed on the holder 16 through the carry-in port 81 or a film formation target 15 in which the substrate and the mask are integrated is carried into the film formation tank 11 from the outside. 17, the carried holder 16 and the film formation target 15 are moved together, temporarily stopped at a position directly above the discharge device 12, and then formed into a film, and then transferred from the carry-out port 82 to the outside of the film formation tank 11. Is configured to do.
  • a loading / unloading chamber (not shown) or another vacuum processing chamber (not shown) is connected to the outside of the carry-in port 81 and the carry-out port 82.
  • the film forming surface on which the organic thin film of the film forming object 15 is formed is directed to the discharge device 12, is located immediately above the discharge device 12, and temporarily stops in a state of facing the discharge plate 36 of the discharge device 12.
  • the vapor of the organic material is discharged from the discharge port 37 of the discharge device 12, the vapor uniformly reaches the film formation surface, and an organic thin film is formed on the film formation surface.
  • the film formation target 15 may be formed by passing the position directly above the discharge device 12 without being stationary.
  • Each of the steam generation devices 13a and 13b includes an exchange device 30, a material supply device 20, an evaporation device 40, a buffer device 50, and a trap device 60, respectively.
  • the exchange device 30 is connected to the material supply device 20, the material supply device 20 is connected to the evaporation device 40, the evaporation device 40 is connected to the buffer device 50, and the buffer device 50 is connected to the switching device 10.
  • the switching device 10 is connected to the trap device 60 and the discharge device 12.
  • the material supply device 20 includes a storage container 21, a hollow cylindrical portion 23, and a linear bar 25.
  • the lower part of the storage container 21 is inclined in a funnel shape, and an opening is formed at the lower end of the funnel-shaped portion.
  • the cylindrical portion 23 is connected to the storage container 21 with the inside communicating with the opening at the lower end thereof.
  • the rod-like body 25 is vertically inserted into the cylindrical portion 23 and the storage container 21.
  • the upper part of the rod-shaped body 25 is located above the funnel-shaped part of the storage container 21, and the lower part is located in the cylindrical part 23.
  • the rod-like body 25 is provided with a spiral projection 26 that extends in the vertical direction while rotating.
  • a powder organic material is disposed in the storage container 21.
  • the distance between the outer periphery of the protrusion 26 and the inner peripheral surface of the cylindrical part 23 is formed to be narrower than the size of the particles of the organic material. It is comprised so that it may not fall through the clearance gap between the parts 23.
  • the organic material when a powdery organic material is disposed in the storage container 21, the organic material is configured to ride on the protrusion 26. However, the spiral inclination of the protrusion 26 causes the rod-like body 25 to be stationary. Since the organic material is formed at an angle at which the organic material does not slide or fall on the projection 26 in the state, the organic material inside the accumulation container 21 passes through the cylindrical portion 23 on the projection 26 when the rod-like body 25 is stationary. Will not fall.
  • the evaporation apparatus 40 has an evaporation tank 41, a through hole is provided in the ceiling of the evaporation tank 41, and the lower end of the cylindrical portion 23 is inserted into the evaporation tank 41 in an airtight manner from the through hole.
  • the lower end of the cylindrical portion 23 is narrowed in a funnel shape, and a drop port 24 is formed at the tip thereof.
  • the internal space of the cylindrical portion 23 and the internal space of the evaporation tank 41 are connected by the drop port 24. ing.
  • the evaporation tank 41 is disposed inside the film formation tank 11.
  • the space between the protrusion 26 and the protrusion 26 has an upper end connected to the internal space of the storage container 21 and a lower end connected to the internal space of the evaporating tank 41 via the internal space of the cylindrical portion 23 and the drop port 24. ing.
  • a rotating device 28 is connected to the rod-shaped body 25, and the rod-shaped body 25 is configured to be rotatable about its vertical central axis. When the rod-shaped body 25 rotates in a predetermined direction, the organic material located on the protrusion 26 is pushed out, falls from the lower end of the gap between the protrusion 26 and the protrusion 26, passes through the tubular portion 23, and evaporates from the dropping port 24 to the evaporation tank 41. Enter inside.
  • the fall amount is proportional to the rotation amount, and the relationship between the fall amount and the rotation amount is obtained in advance.
  • the rod-like body 25 rotates slowly by a rotation amount that drops a necessary amount of organic material with respect to the single film formation target. Accordingly, the organic material is dropped and supplied from the material supply device 20 to the evaporation device 40 little by little.
  • the vapor generation apparatuses 13a and 13b have different chemical structures in the storage containers 21.
  • the organic material of the organic thin film and the organic material of the color former are arranged separately.
  • the content in the organic thin film is greatly different between the base material and the coloring material.
  • the exchange device 30 has an exchange chamber 31 that is a vacuum tank, and the exchange chamber 31 is disposed on the ceiling of the film formation tank 11.
  • a partition valve 29 is provided between the exchange chamber 31 and the film formation tank 11, and the atmosphere in the exchange chamber 31 and the atmosphere in the film formation tank 11 can be connected via the partition valve 29. ing.
  • the storage container 21 is provided with a moving device, and the storage container 21 is configured to be movable up and down together with the cylindrical portion 23 and the rod-shaped body 25.
  • the storage container 21 is disposed in the film forming tank 11 and is located immediately below the partition valve 29.
  • the partition valve 29 When the partition valve 29 is closed, the inside of the film forming tank 11 is in an atmospheric atmosphere.
  • the inside of the film forming tank 11 can be made into a vacuum atmosphere by operating the vacuum exhaust system 19 separated from the film forming tank 11 and connected to the film forming tank 11.
  • the exchange chamber 31 is provided with a door 32. When the door 32 is opened, the exchange chamber 31 can be connected to the atmosphere.
  • An evacuation system 33 is connected to the exchange chamber 31, and the exchange chamber 31 is evacuated by the evacuation system 33 with the partition valve 29 and the door 32 being closed.
  • the storage container 21 located immediately below the partition valve 29 is moved upward together with the cylindrical portion 23 and the rod-shaped body 25, and is allowed to pass through the partition valve 29. 23 and the rod-shaped body 25 are carried into the exchange chamber 31.
  • the partition valve 29 is closed, the inside of the film formation tank 11 is separated from the exchange chamber 31, the vacuum exhaust system 33 is separated from the exchange chamber 31, the atmosphere is introduced into the exchange chamber 31, and the inside of the exchange chamber 31 is at atmospheric pressure. To. At this time, the vacuum atmosphere in the film formation tank 11 is maintained.
  • the door 32 is opened, the inside of the storage container 21 and the air atmosphere are connected by the door 32, and an organic material is put into the storage container 21 in the air atmosphere.
  • the organic material charged into the storage container 21 does not slide or fall on the protrusions 26.
  • the door 32 is closed, the exchange chamber 31 is evacuated by the evacuation system 33, and the exchange chamber 31 is evacuated to a pressure similar to that of the film formation tank 11. .
  • the inside of the storage container 21 and the inside of the cylindrical portion 23 are also evacuated.
  • the partition valve 29 is opened, the storage container 21 is moved into the film formation tank 11 together with the cylindrical portion 23 and the rod-shaped body 25, and the partition container 29 is positioned below the partition valve 29. Close the valve 29.
  • ⁇ Evaporation device> The dropping port 24 described above is located above the bottom surface of the evaporation tank 41, and the organic material dropped from the dropping port 24 of the material supply device 20 collides with the bottom surface of the evaporation tank 41 and is in contact with the bottom surface. Stand still on the bottom.
  • An evaporation heating device 42 for heating the evaporation tank 41 is provided around the evaporation tank 41.
  • the evaporation heating device 42 such as a resistance heating element is connected to a heating power supply 44 and generates heat when energized by the heating power supply 44 to heat the evaporation tank 41.
  • the bottom surface of the evaporation tank 41 is heated by the evaporation heating device 42. Therefore, the bottom surface of the evaporation tank 41 comes into contact with the organic material supplied from the material supply device 20 and heats the organic material. This is a heating unit 43.
  • the organic material has an evaporation temperature that is the temperature at which evaporation starts, and when heated, the organic material does not evaporate immediately even if the temperature is raised to the evaporation temperature, so the organic material is heated to a temperature higher than the evaporation temperature.
  • the evaporation rate increases at higher temperatures, but the higher the temperature, the greater the amount of decomposition.
  • the heat generation of the evaporation heating device 42 is controlled by the amount of current supplied by the heating power supply 44, and the heating unit 43 is set to a vapor generation temperature that is higher than the evaporation temperature of the organic material disposed on the surface thereof. .
  • the vapor generation temperature is so high that no decomposition of the organic material occurs.
  • the organic material on the heating unit 43 is heated to the vapor generation temperature and evaporated to generate an organic material vapor.
  • the organic material supplied from the material supply device 20 is brought into contact with the heating member, and the heating member is heated by the evaporation heating device 42,
  • the heating member serves as the heating unit 43 to generate steam.
  • a material supply amount measuring means 100 for measuring the mass of the organic material dropped from the dropping port 24 may be provided inside the evaporation tank 41.
  • the material supply amount measuring unit 100 includes a material receiving member 101 and a temperature measurement analysis device 102.
  • the temperature measurement analyzer 102 measures the temperature of the material receiving member 101.
  • the material receiving member 101 is heated to a constant temperature by the evaporation heating device 42, but when the organic material falls, the temperature temporarily decreases due to the heat capacity and heat of vaporization of the organic material.
  • a correspondence table is created by measuring the amount of material drop and temperature change in advance.
  • the temperature measurement analysis device 102 calculates the fall amount of the organic material from the temperature of the material receiving member 101 and the correspondence table.
  • the evaporation tank 41 and the discharge device 12 are connected by a connecting pipe 45 (45 1 to 45 3 ), and a buffer device 50 is provided in the middle thereof.
  • the connecting pipe 45 between the buffer device 50 and the discharge device 12 is provided with a switching device 10 composed of a three-way valve.
  • a trap tank 61 of a trap device 60 described later is connected to the switching device 10, and the buffer device 50 is connected to either the discharge device 12 or the trap device 60 by the operation of the switching device 10. It is configured.
  • the buffer device 50 may not be connected to either.
  • the trap tank 61 is connected to the inside of the film forming tank 11 or the vacuum exhaust system 19. Here, it is connected to the inside of the film formation tank 11.
  • the film formation tank 11 is continuously evacuated by the vacuum exhaust system 19 connected to the film formation tank 11, and when the buffer device 50 is connected to the discharge device 12, The evaporation tank 41 is evacuated by the evacuation system 19 through the discharge device 12.
  • the buffer device 50 is evacuated through the trap device 60.
  • the rod-shaped body 25 rotates slowly, and an amount of organic material supplied to one film formation target is supplied to the heating unit 43 little by little.
  • the organic material that has come into contact with the heating unit 43 evaporates in a short time, and the organic material located on the heating unit 43 does not increase.
  • the organic material has a constant evaporation rate. Steam is generated.
  • a backflow prevention gas supply system 49 is connected to the cylindrical portion 23, and a backflow prevention gas is introduced so that vapor generated in the evaporation tank 41 does not enter the storage container 21. Further, the backflow preventing gas suppresses the temperature rise of the cylindrical portion 23, thereby preventing the organic material in the cylindrical portion 23 from being dissolved or sublimated.
  • the backflow prevention gas is heated to a temperature substantially the same as the temperature in the evaporation tank 41.
  • the backflow prevention gas is a rare gas such as argon. Since the pressure in the evaporation tank 41 and the pressure in the film formation tank 11 are lower in the film formation tank 11, the vapor flows out in the direction of the film formation tank 11 together with the backflow preventing gas.
  • the buffer device 50 has a buffer tank 51, one end of connecting pipe 45 1 connected to the opening 48 of the evaporation tank 41, the other end connected to the opening 53 of the buffer tank 51, the connection pipe 45 1 The steam moves toward the buffer tank 51.
  • a heat insulating device 46 is wound around the connecting pipe 45 (45 1 to 45 3 ), and heat is generated by energization from the heat insulating power supply 47.
  • the connecting pipe 45 is an organic material disposed in the steam generating device 13. The temperature is raised to a temperature equal to or higher than the evaporation temperature.
  • a buffer section 52 having a plurality of thin flow paths through which gas flows is arranged inside the buffer tank 51, and when the steam flows in the flow path, the steam collides with the wall surface of the flow path in the buffer section 52.
  • the buffer section 52 has the thin metal wires partially overlapped, and the gap between the thin metal wires is used as the flow path.
  • the buffer section 52 can be configured by stacking a plurality of metal nets.
  • a buffer temperature control device 55 is installed around the buffer tank 51.
  • the buffer power supply 56 energizes the buffer temperature control device 55
  • the buffer temperature control device 55 generates heat, and the buffer tank 51 and the buffer section are heated. And 52 are heated.
  • the temperature of the buffer temperature control device 55 can be controlled by the energization amount of the buffer power source 56. Further, the buffer temperature control device 55 may have means for cooling the buffer unit 52. If the temperature of the buffer layer 51 is set lower than the evaporation temperature of the organic material by the buffer temperature control device 55, the organic material is deposited in the buffer layer 51 and accumulated in the buffer unit 52.
  • the buffer temperature controller 55 is controlled by a detection value of a film thickness sensor 86 described later.
  • the temperature of the buffer unit 52 is raised, and when larger than the desired value, the temperature of the buffer unit 52 is lowered.
  • the gas inlet opening 53 of the buffer tank 51 is covered with a buffer unit 52, and in the buffer unit 52, a gap between the nets and the nets or an overlapping part of the nets is a flow path for the vapor and the backflow preventing gas.
  • the steam flows in the buffer unit 52.
  • the buffer tank 51 an opening 57 is provided for the outflow, one end of the connecting pipe 45 2 is connected to the opening 57, the other end is connected to the switching device 10.
  • the switching device 10 is connected to the main body 35 of the discharge device 12 and the trap tank 61 of the trap device 60 by connecting pipes 45 3 and 69, respectively.
  • the switching device 10 is configured to connect the buffer device 50 to one of the discharge device 12 and the trap device 60, and flows out of the buffer tank 51 when the buffer device 50 is connected to the discharge device 12.
  • the steam thus introduced is introduced into the main body 35 of the discharge device 12 and is introduced into the trap tank 61 of the trap device 60 when connected to the trap device 60.
  • the amount of vapor generated may vary due to fluctuations in the material falling speed.
  • organic materials are powders, it is difficult to drop a certain amount at the same speed.
  • the evaporation rate can be easily controlled and a certain amount of vapor can be supplied.
  • the organic material is accumulated in the buffer device 50 at a temperature close to the evaporation temperature that is equal to or lower than the evaporation temperature, the temperature can be rapidly raised to the evaporation temperature or higher. Further, since the organic material is accumulated in the buffer device 50 for a short time, the organic material is not deteriorated.
  • the organic material is accumulated in the buffer device 50 while the film formation target 15 is replaced, and control is performed so that vapor is released from the buffer device 50 during film formation.
  • steam is supplied from the evaporation device 40, the buffer device 50 is brought to the evaporation temperature or lower, and the buffer device 50 is connected to the trap tank 61 by the switching device 10.
  • the rotational speed of the rotating device 28 is controlled based on the measurement result of the material supply amount measuring means 100.
  • the buffer device 50 is brought to the evaporation temperature or higher, and when the detection value of the film thickness sensor 86 becomes constant, the buffer device 50 is connected to the discharge device 12 by the switching device 10.
  • the buffer temperature control device 55 is controlled by a detection value of a film thickness sensor 86 described later.
  • the vapor may be supplied from the evaporation device 40 to the buffer device 50 at a supply amount slower than the film formation speed, or the vapor from the evaporation device 40 may be stopped. If it is detected from the detection value of the film thickness sensor 86 that the film formation of the specified thickness is completed, the connection destination of the switching device 10 is switched to the trap tank 61, and the temperature of the buffer device 50 is lowered below the evaporation temperature.
  • a cooling medium pipe 63 is wound around the trap tank 61, and the liquid cooling medium cooled from the circulation device 66 is supplied to the cooling medium pipe 63, and the trap tank 61 and the trap unit 62 are connected to the trap apparatus 60. It is cooled to a trap temperature that is lower than the evaporation temperature of the organic material that generated the supplied vapor.
  • the cooling medium flowing through the cooling medium pipe 63 returns to the circulation device 66, is cooled in the circulation device 66, and is supplied again to the cooling medium pipe 63.
  • a waste pipe 68 is connected to the trap tank 61, and a discharge port 67, which is the other end of the waste pipe 68, is disposed in the film forming tank 11.
  • the vapor that comes into contact with the surface of the trap part 62 in the trap tank 61 is deposited on the surface of the trap part 62 and is removed from the gas flowing in the trap tank 61. Accordingly, the gas discharged from the discharge port 67 does not contain much organic material vapor, and most of the gas introduced as the backflow prevention gas is evacuated by the evacuation of the evacuation system 19.
  • the organic material deposited on the trap part 62 can be recovered by taking the trap part 62 out of the trap tank 61 and peeling or re-evaporating it.
  • the film forming apparatus 3 of the present invention does not include the trap device 60, and switches the connection between the discharge device 12 of the buffer device 50 and the waste pipe 68 by the switching device 10.
  • the discharge port 67 at the tip of the disposal pipe 68 can be arranged at a position different from the lower side of the film formation target 15 in the film formation tank 11, or the discharge port can be connected to a vacuum exhaust device (second example).
  • Other configurations are the same as those of the film forming apparatus 2 of FIG.
  • the trap part 62 is spaced apart and arranged with a gap, and is composed of a plurality of metal plates through which steam and backflow prevention gas flow, but a collection of metal fibers and a plurality of metal A net may be laminated. These do not have to be made of metal.
  • a sampling device 84 is attached to a path (here, the connecting pipe 45 2 ) through which the vapor flows between the buffer device 50 and the switching device 10, and the sampling device 84 is provided with a thin film. Vapor before passing through the buffer section 52 and reaching the switching device 10 is extracted from the hole 85 together with the backflow prevention gas, and is connected at a position different from the position where the film formation target 15 passes in the film formation tank 11. some of the tubes 45 within 2 is released.
  • a film thickness sensor 86 is disposed close to the position facing the pore 85, and the gas released from the pore 85 into the film formation tank 11 reaches the film thickness sensor 86, and is in the reaching gas.
  • An organic thin film is formed on the surface of the film thickness sensor 86 by the vapor of the organic material.
  • the relationship between the film thickness of the organic thin film grown on the surface of the film thickness sensor 86 and the film thickness of the organic thin film grown on the film forming object 15 held on the holder 16 and positioned on the discharge device 12 has been examined in advance. Even if the vapor discharged from the buffer device 50 is guided to the trap device 60, the film thickness of the organic thin film formed on the surface of the film thickness sensor 86 is measured by the measurement device 87 connected to the film thickness sensor 86. The film thickness of the organic thin film when the vapor guided to the trap device 60 reaches the surface of the film formation target 15 can be obtained. From the film formation time, the film formation speed on the surface of the film formation target 15 can also be obtained by measurement with the film thickness sensor 86 and the measuring device 87.
  • the temperature of the buffer temperature control device 55 is controlled, and the amount of reevaporation from the buffer device 50 is controlled. Further, the end of film formation is detected based on the detection value of the film thickness sensor 86.
  • the switching device 10 connects the buffer device 50 to the discharge device 12, and then holds one film formation target 15 on the holder 16 and positions it above the discharge device 12.
  • the composition and thickness of the organic thin film formed on the film formation target 15 are determined, and are necessary for forming the organic thin film of one film formation target 15, and are evaporated in the plurality of vapor generating apparatuses 13a and 13b.
  • the rod-shaped body 25 is rotated by the rotating device 28 so that the supply speed becomes a predetermined value, and the organic material on the spiral protrusion 26 moves downward from above in the cylindrical portion 23.
  • the organic material falls into the evaporation tank 41 from the drop port 24 at the lower end of the cylindrical portion 23.
  • the supply speed is a value corresponding to the rotation speed, and the rotation speed is also a value corresponding to the required amount.
  • the generated vapor of each organic material is temporarily stored in the buffer device 50 and re-evaporated, so that the vapor is supplied to the discharge device 12 at a stable supply rate.
  • a composition is formed on the surface of the film formation target 15 with a predetermined film thickness in the film thickness direction. An organic thin film with a predetermined value is formed.
  • the discharge device 12 is provided with a heater 38 and generates heat when energized by a power source 39 to heat the main body 35 and the discharge plate 36.
  • a power source 39 to heat the main body 35 and the discharge plate 36.
  • release apparatus 12 is heated to the temperature more than the highest evaporation temperature among the evaporation temperature of the supplied vapor
  • the film formation target 15 on the discharge device 12 is moved from the discharge device 12 after an organic thin film having a predetermined thickness is formed, and the film formation target that has not been formed is placed on the discharge device 12.
  • the buffer device 50 may be connected to the trap device 60 by the switching device 10 while the film formation target 15 is not disposed on the discharge device 12.
  • the structure of the plurality of vapor generating apparatuses 13a and 13b included in the film forming apparatuses 2 and 3 is the same, but may be different.
  • the organic compound serving as a base material is a vapor generating apparatus 13 c having the same structure as the vapor generating apparatuses 13 a and 13 b of the film forming apparatuses 2 and 3 of the first and second examples. 12 and a vapor generator 14 having an evaporation vessel 71 in which an organic compound 72 as a dopant material is disposed is connected to the same release device 12.
  • An amount of the organic compound 72 which is a dopant material of the vapor generating device 14 is arranged in an evaporation container 71 with respect to a plurality of substrates.
  • the wound evaporator heating device 78 such as a resistance heating element
  • evaporator vessel 71 is connected to the discharge unit 12 by a connecting pipe 45 5.
  • the connection pipe 45 3 which connects the second example deposition apparatus steam generating apparatus 13a, 13b switching device 10 and discharge device 12 shown in a few.
  • the heating power supply 79 energizes the evaporation heating device 78 to generate heat, thereby heating the evaporation container 71.
  • the internal organic compound 72 reaches a temperature equal to or higher than its evaporation temperature, an organic compound vapor is generated inside the evaporation container 71.
  • the switching device 70 is provided consisting of a three-way valve.
  • the switching device 70 is connected to a trap device 60, and by switching the switching device 70, the vapor generated in the evaporation container 71 can be supplied to both the discharge device 12 and the trap device 60. Yes.
  • the trapping device 60 can also prevent the evaporation container 71 from being connected to either.
  • the vapor of the organic compound 72 generated inside the evaporation container 71 is supplied to the discharge device 12.
  • the organic compound vapor generated in the evaporation tank 41 is supplied from the buffer device 50 into the discharge device 12
  • the vapor generated in the evaporation container 71 is supplied to the discharge device 12, and Both vapors generated in the evaporation tank 41 are introduced into the discharge device 12.
  • a carrier gas supply system 73 is connected to the evaporation container 71 so that the vapor generated in the evaporation container 71 can be carried on the carrier gas flow and supplied to the discharge device 12 together with the carrier gas. ing.
  • the switching device 70 blocks the discharge device 12 and the evaporation container 71 and connects the evaporation container 71 to the trap device 90. Can do.
  • the trap device 90 has a trap tank 77, the inside of which is connected to the inside of the film forming tank 11, and is configured to be evacuated by the evacuation system 19. Inside the trap tank 77, a trap portion 96 that comes into contact with steam is provided, and around the trap tank 77, a cooling medium pipe 93 is wound.
  • the cooling medium pipe 93 is connected to the circulation device 92, supplied with a liquid cooling medium cooled from the circulation device 92, and flows through the cooling medium pipe 93.
  • the temperature of the trap tank 77 and the trap section 96 is cooled by the cooling medium flowing in the cooling medium pipe 93 to a trap temperature that is lower than the evaporation temperature of the vapor flowing in the trap tank 77.
  • Each cooling medium pipe 63, 93 and each circulation device 66, 92 constitute a low temperature device.
  • the carrier gas and a very small amount of organic compound vapor emitted from the trap device 90 are evacuated by the evacuation of the evacuation system 19.
  • the organic compound adhering to the trap parts 62 and 96 can be recovered and reused.
  • a film thickness sensor 76 is arranged.
  • the film thickness sensor 76 is connected to the measuring device 74.
  • the sampling device 75 and the film thickness sensor 76 are the same as the sampling device 84 between the buffer device 50 and the switching device 10 and the film thickness sensor 86 that faces the sampling device 84, and the trap device 90 with vapor alone or together with the carrier gas. in a state where it flows and in a part of the steam flowing through the connecting pipe 45 5 is released into the film forming chamber 11 from the pores 95 of the sampling device 75, it reaches the film thickness sensor 76, a thin film on its surface Form. The thickness of the formed film is measured by the measuring device 74, and the film forming speed is obtained from the time of formation. When the determined deposition rate reaches a predetermined value, the dopant vapor can be supplied from the evaporation vessel 71 to the discharge device 12.
  • the film formation target The thin film can be formed on the surface of the object 15.
  • the vapors respectively flowing into the trap devices 60 and 90 from the evaporation container 71 and the buffer device 50 are switched by the switching devices 10 and 70 so as to be supplied to the discharge device 12 together with the carrier gas. 12 and the film formation target 15 face each other while moving still or moving, and an organic thin film to which a dopant is added is formed on the surface of the film formation target 15.
  • the film formation speed is measured by the film thickness sensor 76 and the measuring device 74, and the heating power source 79 is used for evaporation around the evaporation container 71.
  • the dopant is not disposed in the storage container 21, but is disposed in the evaporation container 71.
  • the base material organic compound and the dopant organic compound are mixed. It can also be arranged in the storage container 21. However, it is easier to manage the evaporation rate by arranging the storage container 21 and the evaporation container 71 separately.
  • the base material vapor may flow backward from the connection pipe 45 3 to the connection pipe 45 5 . Since the pressure in the connecting pipe 45 3 to the connecting pipe 45 5 is in the molecular flow region, the reverse flow can be prevented by forming the check baffle 110 in the connecting pipe 45 5 .
  • the adsorption / desorption temperature between multiple steam generators also varies from one steam generator to another depending on the type of organic material, and the optimal variation in steam generation can be achieved according to the type of organic material (chemical structure). It is set to a valid value.
  • one vapor generation device can be connected to one discharge device 12, and in this case, since the organic thin film is formed at a constant film formation rate by the buffer device 50, the film quality is increased in the film thickness direction. Can form a uniform organic thin film.
  • the organic material can be collected by the trap device 60.
  • the number of the nets of the laminated nets per unit area is closer to the far side of the openings 53 and farther from the far side. There are more nets that are the same as the nets or far away. With this arrangement, it is possible to prevent the inside of the buffer device 50 from being blocked during storage.

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JP2011195916A (ja) * 2010-03-23 2011-10-06 Hitachi Zosen Corp 蒸着装置
WO2012039383A1 (ja) * 2010-09-22 2012-03-29 株式会社アルバック 真空処理装置及び有機薄膜形成方法
JP2014031555A (ja) * 2012-08-06 2014-02-20 Kaneka Corp 真空蒸着装置
WO2014027578A1 (ja) * 2012-08-13 2014-02-20 株式会社カネカ 真空蒸着装置及び有機ｅｌ装置の製造方法
JP2014523486A (ja) * 2011-06-22 2014-09-11 アイクストロン、エスイー Ｏｌｅｄの堆積方法および装置
JP2015063724A (ja) * 2013-09-25 2015-04-09 日立造船株式会社 真空蒸着装置
JP2015086451A (ja) * 2013-10-31 2015-05-07 株式会社アルバック 蒸発装置、成膜装置
WO2017189443A1 (en) 2016-04-25 2017-11-02 Innovative Advanced Materials, Inc. Effusion cells, deposition systems including effusion cells, and related methods
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KR102165001B1 (ko) * 2016-05-13 2020-10-13 울박, 인크 유기 박막 제조 장치, 유기 박막 제조 방법
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JP2011195916A (ja) * 2010-03-23 2011-10-06 Hitachi Zosen Corp 蒸着装置
WO2012039383A1 (ja) * 2010-09-22 2012-03-29 株式会社アルバック 真空処理装置及び有機薄膜形成方法
JP2014523486A (ja) * 2011-06-22 2014-09-11 アイクストロン、エスイー Ｏｌｅｄの堆積方法および装置
JP2014031555A (ja) * 2012-08-06 2014-02-20 Kaneka Corp 真空蒸着装置
WO2014027578A1 (ja) * 2012-08-13 2014-02-20 株式会社カネカ 真空蒸着装置及び有機ｅｌ装置の製造方法
CN104540975A (zh) * 2012-08-13 2015-04-22 株式会社钟化 真空蒸镀装置以及有机el装置的制造方法
JPWO2014027578A1 (ja) * 2012-08-13 2016-07-25 株式会社カネカ 真空蒸着装置及び有機ｅｌ装置の製造方法
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JP2015063724A (ja) * 2013-09-25 2015-04-09 日立造船株式会社 真空蒸着装置
JP2015086451A (ja) * 2013-10-31 2015-05-07 株式会社アルバック 蒸発装置、成膜装置
WO2017189443A1 (en) 2016-04-25 2017-11-02 Innovative Advanced Materials, Inc. Effusion cells, deposition systems including effusion cells, and related methods
CN109477200A (zh) * 2016-04-25 2019-03-15 创新先进材料股份有限公司 泻流单元和含有泻流单元的沉积系统以及相关方法
JP2019515132A (ja) * 2016-04-25 2019-06-06 イノベイティブ アドバンスド マテリアルズ，インク．Ｉｎｎｏｖａｔｉｖｅ Ａｄｖａｎｃｅｄ Ｍａｔｅｒｉａｌｓ，Ｉｎｃ． 流出セル、流出セルを含む蒸着システム、及び関連方法
EP3455385A4 (en) * 2016-04-25 2020-02-26 Innovative Advanced Materials, Inc. EFFUSION CELLS, DEPOSITION SYSTEMS WITH EFFUSION CELLS AND RELATED METHODS
CN109477200B (zh) * 2016-04-25 2020-11-27 创新先进材料股份有限公司 泻流单元和含有泻流单元的沉积系统以及相关方法
JP7197364B2 (ja) 2016-04-25 2022-12-27 イノベイティブ アドバンスド マテリアルズ，インク． 流出セル、流出セルを含む蒸着システム、及び関連方法
EP3396731A1 (en) * 2017-04-10 2018-10-31 Samsung Display Co., Ltd. Apparatus and method of manufacturing display apparatus
US11534790B2 (en) 2017-04-10 2022-12-27 Samsung Display Co., Ltd. Apparatus and method of manufacturing display apparatus
JP6959680B1 (ja) * 2020-11-13 2021-11-05 株式会社シンクロン 成膜装置
WO2022102355A1 (ja) * 2020-11-13 2022-05-19 株式会社シンクロン 成膜装置
JP2022078588A (ja) * 2020-11-13 2022-05-25 株式会社シンクロン 成膜装置

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TWI461554B (zh) 2014-11-21
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